Advances in Sample Preparation最新文献_第8页

DES modified silica gel as dispersing material for miniaturized matrix solid phase dispersion applied to triazoles determination DES改性硅胶作为分散材料，用于三唑类化合物的微型基质固相分散测定

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100153

Susanna Della Posta , Valeria Gallo , Emanuele Limiti , Marcella Trombetta , Monica Gherardi , Alessandra Gentili , Laura De Gara , Chiara Fanali

Matrix solid phase dispersion (MSPD) represents one of the most useful methods for pesticides determination in vegetables. This extraction method involves the use of a solid, dispersing material, which is homogenized together with the sample in a mortar and loaded into a cartridge for the analyte's elution with a suitable solvent. Innovative MSPDs involve the use, as dispersing material, of silica gel (SCG) impregnated with deep eutectic solvents (DESs). SCG high porosity can facilitate DES impregnation process due to hydrogen bonds or electrostatic interactions among them.

A miniaturized MSPD extraction for triazoles from tomato using as dispersant DES modified SCG, followed by HPLC-MS extracts analysis, was developed. Four DES modified SCGs were tested in the MSPD procedure and the best result in terms of extracted triazoles was obtained using a choline chloride – Propylene Glycol DES modified SCG. Ethyl Acetate was selected as MSPD procedure extractive solvent resulting more efficient than methanol, acetonitrile and chloroform. The optimization of the extraction procedure involved the study of SCG to DES ratio (w/v), sample to dispersing material ratio (w/w) and extractive solvent volume able to obtain the greatest recovery of triazoles from tomato. The optimized method was validated and maximum values of 3.6 % and 8.3 % were obtained for intra-day and inter-day precision respectively. For each analyte the calculated limit of quantification was similar or lower than their Maximum Residue Limit. Triazoles mean recovery ranged from 70 to 102 %.

The new ChCl-propylene glycol DES modified SCG represents a valid alternative to conventional dispersing material in MSPD procedure apply to pesticides determination.

基质固相分散法（MSPD）是蔬菜中农药含量测定中最有用的方法之一。这种提取方法包括使用固体分散材料，该材料与样品一起在砂浆中均质，并装入一个用合适溶剂洗脱分析物的药筒中。创新的mspd包括使用浸渍有深共晶溶剂（DESs）的硅胶（SCG）作为分散材料。SCG的高孔隙率可以通过氢键或静电相互作用促进DES浸渍过程。研究了以DES改性SCG为分散剂的微型MSPD提取番茄中三唑的方法，并对提取物进行了HPLC-MS分析。用MSPD法对四种DES修饰的SCG进行了测试，氯胆碱-丙二醇DES修饰的SCG提取三唑的效果最好。选择乙酸乙酯作为MSPD萃取溶剂，萃取效率高于甲醇、乙腈和氯仿。优化提取工艺，考察SCG / DES比（w/v）、样品与分散物比（w/w）和萃取溶剂体积对番茄中三唑提取率的影响。对优化后的方法进行了验证，得到的日内精密度最大值为3.6%，日内精密度最大值为8.3%。每种分析物的定量计算限与最大残留限相近或低于其最大残留限。三唑类药物的平均回收率为70% ~ 102%。新型氯丙二醇DES改性SCG代表了一种有效的替代传统分散材料的MSPD方法在农药测定中的应用。

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引用次数: 0

The solvent-assisted dispersive solid-phase extraction method revisited. Application for the determination of anionic surfactants 对溶剂辅助分散固相萃取法进行了研究。阴离子表面活性剂的测定方法

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100162

Serhii Zaruba , Patrycja Makoś-Chełstowska , Vasil Andruch

A new approach in solvent-assisted dispersive solid-phase extraction (SA-DSPE) procedure using a supercooled liquid was developed. It demonstrates the first use of a supercooled liquid in this technique, in particular, and in chemical analysis in general. Moreover, to the best of our knowledge, this is the first work devoted to the determination of the total concentration of anionic surfactants (as LAS, Linear alkylbenzene sulfonate) using a micro-SPE technique. The method is based on the formation of an ion pair between astraphloxine (cationic dye) and an anionic surfactants, with subsequent extraction of the ion pair formed onto a benzophenone sorbent generated in situ after injection of its 5 % solution in an acetone:water 80:20 v/v mixture into an aqueous sample. The resulting turbidness was sedimented by centrifugation. The addition of a few crystals of benzophenone then leads to the solidification of a supercooled solution of the sorbent, which facilitates the separation. Afterwards, the bulk of the aqueous phase was easily decanted, and the resulting sediment was dissolved with 500 μL of acetone; absorbance measurements were carried out in a semi-microcuvette. The calibration plot was linear up to 0.5 µmol L⁻¹ of sodium dodecylbenzene sulfonate (SDBS). The LOD and LOQ, were 9.0 and 30 nmol L^-1 of SDBS, respectively. The developed procedure was applied for the determination of anionic surfactants in various real water samples.

提出了一种利用过冷液体进行溶剂辅助分散固相萃取（SA-DSPE）的方法。它展示了在这种技术中，特别是在化学分析中首次使用过冷液体。此外，据我们所知，这是第一个致力于用微spe技术测定阴离子表面活性剂（如LAS，线性烷基苯磺酸盐）总浓度的工作。该方法是基于在黄芪（阳离子染料）和阴离子表面活性剂之间形成离子对，随后将其在丙酮：水80:20 v/v混合物中注射5%溶液后原位生成的二苯甲酮吸附剂上形成的离子对萃取到含水样品中。所得浊度通过离心沉淀。加入一些二苯甲酮晶体会导致吸附剂的过冷溶液凝固，从而促进分离。之后，将大部分水相轻松滗出，用500 μL丙酮溶解所得沉积物；在半微比色皿中进行吸光度测量。校正图在十二烷基苯磺酸钠（SDBS）浓度为0.5µmol L−1时呈线性关系。sds的LOD和LOQ分别为9.0和30 nmol L-1。该方法可用于各种实际水样中阴离子表面活性剂的测定。

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引用次数: 0

Application of deep eutectic solvents for the determination of inorganic analytes 深共晶溶剂测定无机分析物的应用

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100158

Vasil Andruch , Viera Vojteková , Alina Kalyniukova , Gokhan Zengin , Ingrid Hagarová , Tanya Yordanova

Deep eutectic solvents (DESs), due to their unique physicochemical properties, such as low volatility, tunable viscosity, and excellent solvation capabilities, have emerged as promising alternatives to conventional solvents in the determination of inorganic analytes. This work comprises various DES compositions that effectively improve the sensitivity, selectivity, and environmental sustainability of analytical procedures for the determination of inorganic analytes. DESs crucially take part in extraction, preconcentration, and digestion processes, followed by measurements with atomic absorption spectrometry, plasma-based techniques, UV–Vis spectrophotometry, etc. This work aims to reveal their great potential in the field of elemental analysis for the determination of inorganic analytes in various types of samples. Furthermore, the challenges and limitations associated with the use of DESs, including matrix effects, viscosity issues and compatibility with analytical instrumentation, are critically evaluated.

深共晶溶剂（DESs）由于其独特的物理化学性质，如低挥发性、可调粘度和优异的溶剂化能力，已成为测定无机分析物的传统溶剂的有希望的替代品。这项工作包括各种DES组成，有效地提高了测定无机分析物的分析方法的灵敏度、选择性和环境可持续性。DESs在萃取、预浓缩和消化过程中起着至关重要的作用，随后使用原子吸收光谱法、等离子体技术、紫外可见分光光度法等进行测量。这项工作旨在揭示它们在元素分析领域的巨大潜力，用于测定各种类型样品中的无机分析物。此外，与DESs使用相关的挑战和限制，包括基质效应，粘度问题和与分析仪器的兼容性，进行了批判性评估。

引用次数: 0

Advances in applications of metal-organic frameworks for selective solid-phase extraction and chromatographic separation of active pharmaceutical ingredients 金属-有机骨架在药物活性成分选择性固相萃取和色谱分离中的应用进展

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100151

Zhenyu Song , Bodong Liu , Zezhou Zang , Zeyi Li , Ying Jiang , Tiantian Si , Min Sun

Active pharmaceutical ingredients (APIs) constitute a fundamental component in the development and clinical application of pharmaceuticals, thereby playing an indispensable and pivotal role within the realm of biomedicine. In current research, metal-organic frameworks (MOFs) have garnered considerable attention for studying APIs, serving as effective adsorbents for the extraction of APIs or as stationary phases for their separation. Notably, MOFs composites have significantly enhanced the enrichment and selectivity for APIs by modifying their size, micropore structure, surface characteristics, and charge. The mechanisms underlying these improvements include hydrogen bonding, π-stacking interactions, electrostatic interactions, hydrophobic interactions, and hydrophilic interactions. This comprehensive review focuses on the latest advancements and breakthroughs in the application of MOFs for selective extraction, enrichment, and chromatographic separation of APIs within solid-phase extraction, solid-phase microextraction, and chromatographic stationary phases spanning the period from 2020 to 2024. Additionally, the review highlights the potential development of MOFs in sample preparation chromatographic separation for application, particularly for APIs derived from traditional Chinese medicine (TCM), providing valuable insights into the research and development of nanomaterials such as MOFs in using APIs.

活性药物成分是药物开发和临床应用的基础成分，在生物医学领域中起着不可或缺的关键作用。在目前的研究中，金属有机骨架（MOFs）作为有效的吸附剂用于原料药的提取或作为固定相用于原料药的分离，在原料药的研究中受到了广泛的关注。值得注意的是，mof复合材料通过改变其尺寸、微孔结构、表面特征和电荷，显著提高了原料药的富集和选择性。这些改进的机制包括氢键、π堆积相互作用、静电相互作用、疏水相互作用和亲水相互作用。本文综述了2020年至2024年mof在固相萃取、固相微萃取和色谱固定相中选择性提取、富集和色谱分离原料药的最新进展和突破。此外，本文还强调了mof在样品制备色谱分离中的应用潜力，特别是在中药原料药的应用方面，为mof等纳米材料在原料药应用方面的研究和开发提供了有价值的见解。

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引用次数: 0

Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oils 绿色快速的Fe3O4@Al2O3/AC磁固相微萃取法测定植物油中新烟碱类农药

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100152

Musiiwa V. Sengane , Masixole Sihlahla , Philiswa N. Nomngongo , Nomvano Mketo

A greener sample preparation method based on magnetic solid phase microextraction (MSPμE) was developed for the preconcentration of neonicotinoid pesticides (acetamiprid, imidacloprid, thiacloprid and thiamethoxam) in vegetable oil samples followed by separation and quantification using high performance liquid chromatography with diode array detector (HPLC-DAD). Different characterisation techniques such as Fourier Transform Infrared Spectroscopy (FTIR), Powder X-ray diffraction analysis (PXRD), Thermogravimetric Analysis (TGA), Transmission electron microscopy (TEM), and scanning electron microscope and energy-dispersive X-ray spectroscopy (SEM-EDS) confirmed the synthesised magnetic nano adsorbents (Fe₃O₄, Fe₃O₄@Al₂O₃ and Fe₃O₄@Al₂O₃/AC). The most influential parameters affecting MSPμE of NEOs by Fe₃O₄@Al₂O₃/AC were examined using a multivariate optimisation approach and 8 min extraction time, 13 pH, 9 mg adsorbent mass, and 0.5 mL eluent volume were optimal parameters. The proposed Fe3O4@Al2O3/AC method showed high accuracy (80–119.21%) and precision (≤10 %) for all the investigated NEOs. Additionally, the obtained limit of detection (LOD) ranged from 0.5–1.76 ng µL^-1, the limit of quantification (LOQ) ranged from 1.87–6.62 ng µL^-1 and satisfactory high preconcentration factors (73.02- 407.0) were comparable with literature reported studies. The Analytical GREEness calculator AGREE, BAGI and NEMI analysis confirmed greenness of MSPμE. After that, the validated MSPμE method was applied to real vegetable oil samples (avocado, canola, olive and sunflower), and fortunately, all the investigated NEOs were below LODs of the proposed MSPμE /HPLC-DAD methods.

建立了一种基于磁固相微萃取（MSPμE）的绿色样品制备方法，用于植物油样品中新烟碱类农药（啶虫脒、吡虫啉、噻虫啉和噻虫嗪）的预富集，并采用高效液相色谱二极管阵列检测器（HPLC-DAD）进行分离和定量。不同的表征技术，如傅里叶变换红外光谱（FTIR），粉末x射线衍射分析（PXRD），热重分析（TGA），透射电子显微镜（TEM），扫描电子显微镜和能量色散x射线能谱（SEM-EDS）证实了合成的磁性纳米吸附剂（Fe3O4， Fe3O4@Al2O3和Fe3O4@Al2O3/AC）。采用多元优化方法考察了Fe3O4@Al2O3/AC法提取neo的MSPμE的影响因素，确定提取时间为8 min， pH为13，吸附剂质量为9 mg，洗脱液体积为0.5 mL。所提出的Fe3O4@Al2O3/AC方法对所研究的近地天体具有较高的准确度（80-119.21%）和精密度（≤10%）。检出限（LOD）为0.5 ~ 1.76 ngµL-1，定量限（LOQ）为1.87 ~ 6.62 ngµL-1，高富集系数（73.02 ~ 407.0）与文献报道的研究相当。分析绿色计算器AGREE、BAGI和NEMI分析证实了MSPμE的绿色度。然后，将验证的MSPμE方法应用于实际植物油样品（牛油果、菜籽油、橄榄和向日葵），幸运的是，所有检测的neo都低于所建立的MSPμE /HPLC-DAD方法的lod。

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引用次数: 0

New trends in bioanalysis sampling and pretreatment: How modern microsampling is revolutionising the field 生物分析采样和预处理的新趋势：现代微采样如何彻底改变该领域

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100161

Michele Protti , Elisa Milandri , Roberta Di Lecce , Laura Mercolini , Roberto Mandrioli

Microsampling technologies are revolutionising bioanalysis by enabling minimally invasive, decentralized sample collection, offering significant advantages over traditional methods in terms of patient compliance, cost-effectiveness, and analytical efficiency. This review explores the latest advancements in microsampling devices, including microfluidic and quantitative dried blood spot systems (mfDBS and qDBS, respectively), calibrated capillary-based devices, volumetric absorptive microsampling (VAMS) technologies, microneedle-based microsampling, radial-based DBS devices, membrane-based plasma separation technologies and vacuum-assisted blood collection systems. By addressing pre-analytical variability, enhancing analyte stability, and supporting decentralized workflows, these technologies align with modern and green analytical chemistry principles. The unique capabilities of these emerging microsampling technologies and devices further demonstrate their transformative potential. However, challenges remain, including haematocrit dependency for some parameters, user variability, and standardisation across devices. This review highlights ongoing innovations and their implications for expanding to high-quality bioanalytical testing.

微采样技术通过实现微创、分散的样本采集，正在彻底改变生物分析，在患者依从性、成本效益和分析效率方面比传统方法具有显着优势。本文综述了微采样设备的最新进展，包括微流控和定量干血点系统（分别为mfDBS和qDBS），校准毛细管设备，体积吸收微采样（VAMS）技术，微针微采样，径向DBS设备，膜等离子体分离技术和真空辅助采血系统。通过解决分析前的可变性，增强分析物的稳定性，并支持分散的工作流程，这些技术符合现代和绿色分析化学原则。这些新兴的微采样技术和设备的独特功能进一步展示了它们的变革潜力。然而，挑战仍然存在，包括对某些参数的红细胞压积依赖，用户可变性和跨设备的标准化。这篇综述强调了正在进行的创新及其扩展到高质量生物分析测试的意义。

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引用次数: 0

Development of an automated sorptive extraction system for trace analysis in water 用于水中痕量分析的自动吸附萃取系统的研制

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100156

Frank Jacobs , Dr. Klaus Kerpen , Dr. Eike Kleine-Benne , PD Dr. Ursula Telgheder

Stir bar sorptive extraction (SBSE) is an established microextraction technique developed in the early 2000s. It has gained widespread use in laboratories around the world, but always had one drawback in that it was a manual sample preparation technique. The newly developed system presented in this study aims to combine the well-known characteristics of SBSE with fully automated sample preparation. The presented system is based on a novel sample probe design, which uses the same dimensions and materials of sorbent phase as the commercially available Gerstel Twister® SBSE technology. To test the performance of this system, pesticides were extracted from pure water as well as river water. Limits of detection (4.5 ng/L to 53.6 ng/L) and quantification (15.7 ng/L to 327.6 ng/L) as well as standard method deviation (3.2 % to 37.6 %) were determined for 21 pesticides based on DIN EN ISO 27,108, part of the water framework directive (WFR). Standard addition was used to quantify pesticides in river water matrix. To check the performance of the new development, it was compared to established methods like manual SBSE, thin film micro extraction (TFME) and SPME-Arrow. The results are comparable between automated sorptive extraction (ASE) and SBSE (average of 84 % compared to automated system), as expected. Performance compared to TFME (65 %) and SPME-Arrow (3 %) was significantly better, especially to the latter. These results show that the automated sorptive extraction system developed in this paper is competitive with already established techniques.

搅拌棒吸附萃取（SBSE）是21世纪初发展起来的一种成熟的微萃取技术。它在世界各地的实验室中得到了广泛的应用，但一直有一个缺点，那就是它是一种手工样品制备技术。本研究中提出的新开发的系统旨在将SBSE众所周知的特性与全自动样品制备相结合。提出的系统是基于一种新的样品探针设计，它使用相同的尺寸和材料的吸附剂相作为市售的Gerstel Twister®SBSE技术。为了测试该系统的性能，分别从纯净水和河水中提取农药。根据水框架指令（WFR）的一部分DIN EN ISO 27,108，确定了21种农药的检出限（4.5 ng/L ~ 53.6 ng/L）、定量限（15.7 ng/L ~ 327.6 ng/L）和标准方法偏差（3.2% ~ 37.6%）。采用标准添加法对河流水基质中农药进行定量分析。为了检查新开发的性能，将其与现有的方法（如手动SBSE，薄膜微萃取（TFME）和SPME-Arrow）进行比较。结果与预期的一样，自动吸附萃取（ASE）和SBSE（与自动化系统相比平均为84%）之间具有可比性。与TFME（65%）和SPME-Arrow（3%）相比，性能明显更好，尤其是后者。这些结果表明，本文开发的自动吸附萃取系统与已有的技术相比具有竞争力。

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引用次数: 0

Vial-coated thin film microextraction for perfluoroalkyl carboxylic acids (PFCAs) determination in water by GC–MS 气相色谱-质谱法测定水中全氟烷基羧酸（PFCAs）

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100147

J․Mabel Luna-Díaz , Luz O․ Leal-Quezada , Laura Ferrer , Edwin Palacio

Perfluoroalkyl carboxylic acids (PFCAs), a subclass of perfluoroalkyl substances (PFAs) commonly detected in water, are of increasing concern due to their persistence, bioaccumulative nature, and harmful effects on health. Determining PFCAs in environmental matrices is challenging because they are typically present at ng L⁻¹ levels and tend to adsorb onto materials like filtration membranes, causing significant losses during analysis. To address these challenges, a thin-film microextraction (TFME)-coated vial was designed for PFCA (C5–C10) extraction, coupled with gas chromatography-mass spectrometry (GC–MS). Glass was selected as the support material due to its low adsorption rate and superior chemical resistance compared to other polymers. The TFME coating, made from a weak anion exchange resin and polyacrylonitrile (10 % w/w) as a binder polymer, effectively extracts analytes from complex matrices while minimizing co-extraction of interfering macromolecules. The method eliminates the need for sample filtration, preventing PFCA loss in filtration membranes. Under optimal conditions, the extraction efficiency ranged from 70 to 100 %. Detection and quantification limits were 0.13–2.1 ng L⁻¹ and 0.42–7.1 ng L⁻¹, respectively. Intra- and inter-assay relative standard deviations (% RSD) were 4.9–2.2 % and 4.8–2.3 %, respectively, with a linear working range of 10–1000 ng L⁻¹ for the TFME-coated device. This method is suitable for PFCA determination in drinking water and complies with the Directive 2020/2184, which sets a maximum allowable limit of 500 ng L⁻¹ for total PFAs.

全氟烷基羧酸（PFCAs）是常见于水中的全氟烷基物质（PFAs）的一个亚类，由于其持久性、生物蓄积性和对健康的有害影响而日益受到关注。测定环境基质中的PFCAs具有挑战性，因为它们通常以ng L -¹的水平存在，并且倾向于吸附在过滤膜等材料上，在分析过程中造成重大损失。为了解决这些挑战，设计了一种薄膜微萃取（TFME）包被的小瓶，用于PFCA （C5-C10）的提取，并结合气相色谱-质谱（GC-MS）。与其他聚合物相比，玻璃的吸附率低，耐化学性好，因此选择玻璃作为支撑材料。TFME涂层由弱阴离子交换树脂和聚丙烯腈（10% w/w）作为粘合剂聚合物制成，可以有效地从复杂基质中提取分析物，同时最大限度地减少干扰大分子的共萃取。该方法消除了样品过滤的需要，防止了PFCA在过滤膜中的损失。在最佳条件下，提取效率为70% ~ 100%。检测限和定量限分别为0.13-2.1 ng L⁻¹和0.42-7.1 ng L⁻¹。测定内和测定间的相对标准偏差（% RSD）分别为4.9 - 2.2%和4.8 - 2.3%，线性工作范围为10-1000 ng L - 1。本方法适用于饮用水中PFCA的测定，符合指令2020/2184，该指令规定了PFAs总量的最大允许限量为500 ng L - 1。

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引用次数: 0

Towards eco-metabolomics: NADES-guided extraction enables semi-quantitative metabolomics for Melissa officinalis 走向生态代谢组学：nades引导提取实现了药用草的半定量代谢组学

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100154

Chiara Spaggiari , Isa Sara Aimee Hiemstra , Antoinette Kazbar , Gabriele Costantino , Laura Righetti

In recent years, there has been a growing emphasis on the development of green extraction techniques that minimize environmental impact while maximizing yield of the extracted compounds. To this aim, in this study we investigated the potential of green solvents for extracting bioactive compounds from Melissa officinalis (MO) leaves. Specifically, we focus on the application of 20 Natural Deep Eutectic Solvents (NADES) with a relative polarity ranging from 0.34 to 1.29. Their extraction affinity against a set of 11 plant metabolites was predicted using COSMO-RS software and experimentally validated using quantitative LCHRMS analysis. Subsequently, the same extracts were subjected to non-target metabolomics to uncover the NADES selectivity towards the wide spectrum of MO leaf metabolites. Data preprocessing and feature alignment were performed using MZmine, and aligned features were annotated using SIRIUS+CSI:FingerID.

Overall, 249 and 195, metabolites were annotated in positive and negative ionization ion mode, respectively. Additionally, to have a more accurate view of the different NADES extraction capacity, we adopted a semi-quantitative approach that enables the prediction of concentration for all the annotated metabolites (N = 444).

The results highlighted the selectivity of some NADES in extracting very diverse biochemical classes, providing valuable insights into the composition and concentration of bioactive compounds. Interestingly, thymol-menthol NADES demonstrated the ability to efficiently extract a broad range of bioactive compounds, yielding a metabolome comparable to that obtained with conventional ethanolic. Overall, the entire workflow facilitated the green extraction and annotation of known bioactive molecules that had never been described in MO.

近年来，人们越来越重视绿色提取技术的发展，以尽量减少对环境的影响，同时最大限度地提高提取化合物的产量。为此，本研究探讨了绿色溶剂提取梅丽莎叶中生物活性物质的潜力。具体来说，我们重点研究了20种相对极性在0.34 ~ 1.29之间的天然深共晶溶剂（NADES）的应用。利用cosmoo - rs软件预测了它们对11种植物代谢物的提取亲和力，并通过定量LCHRMS分析进行了实验验证。随后，对相同的提取物进行非靶代谢组学研究，以揭示NADES对MO叶代谢物的广谱选择性。使用MZmine进行数据预处理和特征对齐，对齐后的特征使用SIRIUS+CSI:FingerID进行标注。总的来说，249和195种代谢物分别以正离子和负离子模式标注。此外，为了更准确地了解不同的NADES提取能力，我们采用了半定量方法，可以预测所有注释代谢物的浓度（N = 444）。结果突出了一些NADES在提取非常不同的生化类中的选择性，为生物活性化合物的组成和浓度提供了有价值的见解。有趣的是，百里香薄荷醇NADES能够有效地提取广泛的生物活性化合物，产生与传统乙醇相当的代谢组。总的来说，整个工作流程促进了MO中从未描述过的已知生物活性分子的绿色提取和注释。

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引用次数: 0

Electrospun chitosan modified montmorillonite/polyvinyl alcohol nanofibers as suitable coating for fiber-in-tube solid-phase microextraction of trace amounts of tricyclic antidepressants in biological fluids 静电纺壳聚糖改性蒙脱土/聚乙烯醇纳米纤维涂层用于管中纤维固相微萃取生物体液中微量三环类抗抑郁药

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2024.100145

Saeed Pourhosseini, Yadollah Yamini, Seyedeh Sara Nasrollahi

Chitosan intercalated montmorillonite and polyvinyl alcohol-citric acid (PVA/CA) nanofibers were electrospun onto stainless steel wires. The fibers were placed inside a stainless steel tube and utilized for fiber-in-tube solid phase microextraction (FIT-SPME) to detect trace levels of tricyclic antidepressant drugs (TCAs) in biological samples. The analytes were separated and quantified using gas chromatography coupled with mass spectrometric detection (GC–MS). The effects of various parameters on the extraction efficiency, including pH (9), extraction time (25 min), extraction flow rate (3 mL min^-1), salt addition (0 % w/v), type of eluent (ethanol 99 %), eluent volume (300 µL), and desorption flow rate (70 µL min^-1), were investigated and optimized. Under optimal conditions, the linear dynamic range for doxepin, and sertraline was found to be 0.08–750.0 ng mL^-1; for amitriptyline, desipramine, and trimipramine, it was 10.0–750.0 ng mL^-1; and for carbamazepine and maprotiline, it was 50.0–750.0 ng mL^-1. The proposed method exhibited low limits of detections in the range of 0.02–15.2 ng mL^-1. Additionally, coefficients of determination (R²) exceeding 0.9911 were achieved, indicating excellent linearity for the calibration curves. To assess the feasibility of the FIT-SPME-GC–MS method, extraction and analysis of TCAs were performed on plasma and urine samples. Relative recovery percentages (RR%) ranged from 90.3 % to 117.6 %.

将壳聚糖嵌层蒙脱土和聚乙烯醇-柠檬酸（PVA/CA）纳米纤维电纺成不锈钢丝。这些纤维被放置在一个不锈钢管中，用于纤维管固相微萃取（FIT-SPME），以检测生物样品中痕量的三环抗抑郁药物（TCAs）。采用气相色谱-质谱联用检测（GC-MS）对分析物进行分离和定量。考察了pH(9)、提取时间（25 min）、提取流量（3 mL min-1）、盐添加量（0% w/v）、洗脱液类型（99%乙醇）、洗脱液体积（300µL）、解吸流量（70µL min-1）等参数对提取效率的影响，并进行了优化。在最佳条件下，多塞平和舍曲林的线性动态范围为0.08 ~ 750.0 ng mL-1；阿米替林、地西帕明和三嗪帕明为10.0 ~ 750.0 ng mL-1；卡马西平和马普替林为50.0 ~ 750.0 ng mL-1。该方法的低检出限为0.02 ~ 15.2 ng mL-1。测定系数（R²）均大于0.9911，表明标定曲线线性良好。为了评估FIT-SPME-GC-MS方法的可行性，对血浆和尿液样本进行了TCAs的提取和分析。相对回收率（RR%）为90.3% ~ 117.6%。

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引用次数: 0